US4908133A - Process for working up aqueous electrolyte-containing suspensions of highly swellable layer silicates - Google Patents

Process for working up aqueous electrolyte-containing suspensions of highly swellable layer silicates Download PDF

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Publication number
US4908133A
US4908133A US07/343,467 US34346789A US4908133A US 4908133 A US4908133 A US 4908133A US 34346789 A US34346789 A US 34346789A US 4908133 A US4908133 A US 4908133A
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Prior art keywords
electrolyte
membrane filtration
pipe
suspension
concentrate
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Expired - Fee Related
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US07/343,467
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English (en)
Inventor
Willi Wuest
Norbert Kuehne
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Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Assigned to HENKEL KOMMANDITGESELLSCHAFT AUF AKTIEN (HENKEL KGAA), HENKELSTRASSE 67, POSTFACH 1100, D-4000 DUESSELDORF 1, GERMANY A CORP. OF FEDERAL REPUBLIC OF GERMANY reassignment HENKEL KOMMANDITGESELLSCHAFT AUF AKTIEN (HENKEL KGAA), HENKELSTRASSE 67, POSTFACH 1100, D-4000 DUESSELDORF 1, GERMANY A CORP. OF FEDERAL REPUBLIC OF GERMANY ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: KUEHNE, NORBERT, WUEST, WILLI
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/40—Clays
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/40—Clays
    • C01B33/405—Clays not containing aluminium

Definitions

  • This invention relates to a process for working up aqueous electrolyte-containing suspensions of highly swellable layer silicates.
  • the mother liquor is first separated off by filtration in filter presses, particularly membrane filter presses.
  • the layer silicates remain in the filter cake as a gel-like mass together with part of the adhering mother liquor of high electrolyte content.
  • the layer silicates begin to swell considerably, clogging the pores of the filter medium so that filtration becomes very difficult or even impossible. Because of these difficulties, the layer silicates can only be worked by a very laborious and complicated filtration and washing process.
  • this object is achieved by a continuous multistage membrane filtration process for working up an aqueous electrolyte-containing suspension of highly swellable layer silicates comprising the steps of (1) passing said suspension through a membrane filtration stage to from a retentate composed of said concentrate wherein said concentrate contains said highly swellable layer silicate and a portion of said electrolyte, the remaining portion of said electrolyte being present in said permeate; (2) diluting said concentrate with deionized water to form a slurry, and (3) recycling said slurry to step (1) and (2) and continuing said recycling until an electrolyte-free layer silicate suspension is produced.
  • FIG. 1 illustrates a simplified flow chart of a continuous membrane filtration process.
  • FIG. 2 illustrates a simplified flow chart of a discontinuous or batch-wise membrane filtration process.
  • the layer silicates can be isolated from the starting suspension almost completely free from electrolyte by membrane filtration.
  • the layer silicates are isolated in the retentate with a portion of the electrolyte passing through the membrane in an aqueous solution in the permeate.
  • the concentrate cannot settle over the pores as in filter presses, so that electrolyte-containing permeate can pass through the pores at any time.
  • the filtration time is negligible compared with the time required for working up in filter presses.
  • the process can be operated in a continuous manner wherein the starting suspension is continuously delivered to the successive membrane stages.
  • the layer silicates worked up may be aftertreated or processed as required without interruption.
  • the process may also be operated in a batch-wise manner wherein the starting suspension may be delivered discontinuously from a storage container to one or more membrane stages connected in parallel, the concentrate from the individual stages may be collected in a collecting container and diluted therein with fully deionized water and the diluted concentrate may then be subjected to further purifications in the membrane stages with recycling and dilution in each stage.
  • This variant of the process is particularly suitable when the layer silicates worked up are to be subsequently processed after a time interval or in batches.
  • each membrane stage is formed by a plurality of membrane modules arranged one behind the other. This arrangement of several modules in series provides for adequate filtration.
  • the membrane filtration is carried out at crossflow rates of from 3 to 6 m/s and preferably at crossflow rates of from 4 to 4.5 m/s.
  • the membrane filtration is carried out at temperatures in the range from 20° to 200° C. and preferably at temperatures in the range from 80° to 140° C.
  • the exact temperature to be established depends on the properties of the layer silicates to be worked up.
  • the membrane filtration is carried out under pressures on the permeate side of the order of 16 bar on entry into each membrane stage.
  • a pressure such as this provides for optimal filtration.
  • the membrane filtration is carried out under pressures on the permeate side above the particular steam pressure. Carrying out the process in this way ensures that, at temperatures above 100° C. on the permeate side, no evaporation of water can occur to the detriment of filtration.
  • the starting suspension is filtered in a filter press before working up by membrane filtration. Most of the mother liquor of the starting suspension is separated off in this filter press before working up actually begins.
  • the electrolyte-free suspension is dried by spray drying after membrane filtration.
  • FIG. 1 which illustrates a simplified flow chart of a continuous membrane filtration process
  • the process encompasses a storage container 1 to which an aqueous electrolyte-containing suspension of highly swellable layer silicates is delivered through a pipe 2.
  • a pipe 3 in which a pump 4 is arranged leads off from the storage container 1.
  • the pipe 3 opens into a first membrane stage 5 consisting of two modules 6 and 7 arranged one behind the other, the concentrate from the module 6 being delivered to the module 7 through a pipe 8.
  • the permeate from the modules 6 and 7 is run off through two permeate pipes 9 and 10 into a central permeate pipe 11.
  • a concentrate pipe 12 Arranged where the concentrate (retentate) leaves the module 7 of the first stage 5 is a concentrate pipe 12 into which opens a pipe 13 branching off from a central water pipe 14 through which fully deionized water is delivered.
  • the pipe 12 leads through a pump 15 into a second membrane stage 16 consisting of two modules 17 and 18 arranged one behind the other.
  • a pipe 21 is connected on the permeate side of the module 18 and a pipe 22 on the concentrate side.
  • the central water pipe 14 opens into the pipe 22.
  • the pipe 22 leads through a pump 23 into a third membrane stage 24 formed by two modules 25 and 26.
  • a concentrate pipe 27 which opens into the module 26, and a permeate pipe 28 which leads into the central permeate pipe 11.
  • a product pipe 29 leads off from the module 26 on the concentrate side while a pipe 30 which opens into the central permeate pipe 11 leads off therefrom on the permeate side.
  • the aqueous, electrolyte-containing starting suspension of highly swellable layer silicates is continuously delivered to the first membrane stage 5 from the storage container 1 through the pipe 3 and the pump 4.
  • part of the aqueous electrolyte is filtered off and removed through the permeate pipe 9.
  • the concentrated layer silicates then pass through the concentrate pipe 8 into the second module 7 where they are further concentrated, aqueous electrolyte being filtered off as permeate and removed through the pipe 10.
  • the still just pumpable concentrate with an already distinctly reduced electrolyte content is then diluted with fully deionized water from the pipe 13 to improve its pumpability and is delivered by the pump 15 into the second membrane stage 16.
  • the electrolyte-containing permeate filtered off is again removed through the permeate pipes 20 and 21.
  • the still pumpable concentrate of the module 18 already has a very low electrolyte content at this stage.
  • the concentrate containing the layer silicates is delivered to a third membrane stage 24.
  • the concentrate issuing from the second membrane stage 16 through the pipe 22 is first mixed with fully deionized water through the pipe 14 to improve its pumpability and is delivered by the pump 23 into the membrane stage 24.
  • the layer silicates are then further worked up in the modules 25 and 26. Residual electrolyte is removed from the modules 25 and 26 on the permeate side through the pipes 28 and 30.
  • the concentrate issuing from the module 26 through the pipe 29 now consists of a completely electrolyte-free layer silicate suspension. This electrolyte-free suspension may then be delivered through the pipe 29 to a drying stage or the like although this is not shown in the drawing.
  • a discontinuous or batch-wise membrane filtration plant is shown in FIG. 2.
  • a storage vessel 31 for holding the electrolyte-containing starting suspension of highly swellable layer silicates comprises an outlet pipe 32 in which a pump 33 is arranged.
  • Two parallel branch pipes 34 and 35 with pumps 36 and 37 lead off from the pipe
  • the branch pipes 34 and 35 open into two membrane stages 38 and 39 connected in parallel which each consist of two modules 40,41 and 42,43 arranged one behind the other.
  • a permeate pipe 44 leads off from the first module 40 of the first membrane stage 38 while another permeate pipe 45 leads off from the second module 41, the two permeate pipes 44 and 45 opening into the central permeate pipe 46.
  • the concentrate of the module 40 passes through a concentrate pipe 47 into the second module 41 of which the concentrate issues through a pipe 48.
  • the second membrane stage 39 comprises a permeate pipe 49 on the first module 42 and a permeate pipe 50 on the second module 43.
  • the concentrate of the module 42 passes through a pipe 51 into the second module 43 of which the concentrate enters the pipe 32 through a pipe 52.
  • the pipe 32 After the opening of the pipe 52, the pipe 32 assumes the form of a return pipe 53 and opens into the storage container 31.
  • the storage container 31 has a feed pipe 54 for fully deionized water.
  • the aqueous, electrolyte-containing starting suspension of highly swellable layer silicates is delivered from the storage container 31 through the pipe 32 by the pump 33, the pump 33 being switched off after emptying of the container 31.
  • the starting suspension is then pumped through the branch pipes 34 and 35 and the pumps 36 and 37 into the parallel membrane stage 38 and 39.
  • the suspension is first concentrated in the first module 40, 42 of which the aqueous electrolyte-containing permeate is removed through the pipes 44 and 49 into the central permeate pipe 46.
  • the layer silicates in the concentrate are passed through the pipes 47 and 51 into the second modules 42 and 43 and further concentrated therein.
  • the electrolyte-containing permeate issues through the permeate pipes 45 and 50 while the concentrate containing the layer silicates is removed through the pipes 48 and 52 and delivered to the return pipe 53.
  • the still pumpable, concentrated suspension then passes through the return pipe 53 back into the storage container 31 which now serves as a collecting container.
  • the worked-up suspension may then be removed from the collecting container 31 and further processed.
  • the storage or collecting container 31 thus emptied may then be filled with another electrolyte-containing starting suspension.
  • a membrane stage may also be formed by more than two modules arranged one behind the other.
  • the number of membrane stages used may be adapted to the particular application.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
US07/343,467 1988-04-30 1989-04-26 Process for working up aqueous electrolyte-containing suspensions of highly swellable layer silicates Expired - Fee Related US4908133A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3815008A DE3815008A1 (de) 1988-04-30 1988-04-30 Verfahren zur aufarbeitung waessriger, elektrolyte enthaltender suspensionen hochquellfaehiger schichtsilicate
DE3815008 1988-04-30

Publications (1)

Publication Number Publication Date
US4908133A true US4908133A (en) 1990-03-13

Family

ID=6353497

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US07/343,467 Expired - Fee Related US4908133A (en) 1988-04-30 1989-04-26 Process for working up aqueous electrolyte-containing suspensions of highly swellable layer silicates

Country Status (6)

Country Link
US (1) US4908133A (de)
EP (1) EP0340544B1 (de)
JP (1) JPH0214810A (de)
BR (1) BR8902034A (de)
DE (2) DE3815008A1 (de)
NO (1) NO891778L (de)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6187200B1 (en) * 1994-10-12 2001-02-13 Toray Industries, Inc. Apparatus and method for multistage reverse osmosis separation
FR2817488A1 (fr) * 2000-12-05 2002-06-07 Eastman Kodak Co Procede de purification d'un melange de particules colloidales d'aluminosilicates
US20030141250A1 (en) * 2002-01-18 2003-07-31 Masahiro Kihara Desalination method and desalination apparatus
US6645383B1 (en) * 2000-08-25 2003-11-11 Usf Consumer & Commercial Watergroup, Inc. Process and apparatus for blending product liquid from different TFC membranes
US20090223881A1 (en) * 2008-03-04 2009-09-10 Peter Villeneuve Reverse Osmosis System with Dual Water Intake
US20130032540A1 (en) * 2010-03-04 2013-02-07 Terragroup Corporation Lightweight modular water purification system with reconfigurable pump power options

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3821516A1 (de) * 1988-06-25 1989-12-28 Henkel Kgaa Verfahren zum entsalzen quellfaehiger schichtsilikate

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4279879A (en) * 1979-10-01 1981-07-21 W. R. Grace & Co. Silica gel

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL171535C (nl) * 1977-10-27 1983-04-18 Wafilin Bv Inrichting voor membraanfiltratie.
US4610792A (en) * 1985-01-14 1986-09-09 Memtek Corporation Membrane filtration process
CH668961A5 (de) * 1986-02-07 1989-02-15 Ciba Geigy Ag Verfahren zur reinigung von farbstoffhaltigen abwaessern.
HU200563B (en) * 1987-03-06 1990-07-28 Laszlo Szuecs Method and apparatus for treating liquids consist of foreign matter by diaphragm filter device

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4279879A (en) * 1979-10-01 1981-07-21 W. R. Grace & Co. Silica gel

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6187200B1 (en) * 1994-10-12 2001-02-13 Toray Industries, Inc. Apparatus and method for multistage reverse osmosis separation
US6645383B1 (en) * 2000-08-25 2003-11-11 Usf Consumer & Commercial Watergroup, Inc. Process and apparatus for blending product liquid from different TFC membranes
FR2817488A1 (fr) * 2000-12-05 2002-06-07 Eastman Kodak Co Procede de purification d'un melange de particules colloidales d'aluminosilicates
EP1219341A1 (de) * 2000-12-05 2002-07-03 Eastman Kodak Company Verfahren zum Trennen einer Mischung von kolloidalen Aluminosilicatteilchen
US6685836B2 (en) 2000-12-05 2004-02-03 Eastman Kodak Company Method for separating a mixture of colloidal aluminosilicate particles
US20030141250A1 (en) * 2002-01-18 2003-07-31 Masahiro Kihara Desalination method and desalination apparatus
US20090223881A1 (en) * 2008-03-04 2009-09-10 Peter Villeneuve Reverse Osmosis System with Dual Water Intake
US20130032540A1 (en) * 2010-03-04 2013-02-07 Terragroup Corporation Lightweight modular water purification system with reconfigurable pump power options

Also Published As

Publication number Publication date
EP0340544A3 (de) 1991-07-24
DE3815008A1 (de) 1989-11-09
EP0340544A2 (de) 1989-11-08
NO891778D0 (no) 1989-04-28
JPH0214810A (ja) 1990-01-18
EP0340544B1 (de) 1993-08-04
NO891778L (no) 1989-10-31
DE58905099D1 (de) 1993-09-09
BR8902034A (pt) 1989-12-05

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Owner name: HENKEL KOMMANDITGESELLSCHAFT AUF AKTIEN (HENKEL KG

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNORS:WUEST, WILLI;KUEHNE, NORBERT;REEL/FRAME:005146/0314

Effective date: 19890421

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Effective date: 19940313

STCH Information on status: patent discontinuation

Free format text: PATENT EXPIRED DUE TO NONPAYMENT OF MAINTENANCE FEES UNDER 37 CFR 1.362